CN104404288A - Method for preparing light Nb-Ti-Al based porous material - Google Patents
Method for preparing light Nb-Ti-Al based porous material Download PDFInfo
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- CN104404288A CN104404288A CN201410677820.4A CN201410677820A CN104404288A CN 104404288 A CN104404288 A CN 104404288A CN 201410677820 A CN201410677820 A CN 201410677820A CN 104404288 A CN104404288 A CN 104404288A
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Abstract
The invention provides a method for preparing a light Nb-Ti-Al based porous material, and belongs to the technical field of powder metallurgy porous materials. The method comprises the following process procedures: firstly, performing high energy ball milling on niobium powder, titanium powder, aluminum powder and element powder of other alloy elements to obtain mechanical alloyed powder; uniformly mixing Nb-Ti-Al based alloy powder with rotating electrode atomized niobium alloy powder through ball milling and forming at the pressure of 200-700 MPa to obtain a formed blank; performing vacuum pressure-free sintering and thermal treatment on the formed blank to obtain the Nb-Ti-Al based porous material. Pores are formed by virtue of the Kirkendall effect that pores are formed in a substrate because of partial diffusion of the Al element, and the strength of a porous body is improved with the combination of a sintered neck formed by the atomized alloy powder. The light Nb-Ti-Al based porous material is simple in preparation process, and the porous structure is easy to control.
Description
Technical field
The invention belongs to powder metallurgy porous material technical field, specifically provide a kind of method preparing lightweight Nb-Ti-Al based porous materials.
Background technology
The density of niobium in refractory metal is minimum, can reduce the density of niobium alloy in niobium matrix after adding the strengthening elements such as Ti, Al further, and maintain that niobium-base alloy fusing point is high, mechanical behavior under high temperature and the feature such as welding property is excellent.Nb-Ti-Al based porous materials is a kind of structure-function integrated material of lightweight, its use temperature is greater than 1200 DEG C, have higher use temperature than the nickel-base alloy porous material used at present and TiAl intermetallic compound porous material, the fields such as the support of the catalyst used under the high temperature conditions, strainer and heat exchanger have important application prospect.The preparation method of niobium alloy porous material mainly contains the method such as loose powder sintering method, foam impregnation method.Loose powder sintering method is more difficult prepares highly porous, the uniform porous niobium of pore radiuses and distribution.Foraminous die plate containing powder slurries for carrier with polyurethane foam or other foraminous die plate, first with niobium or niobium alloy powder impregnating slurry foraminous die plate, is then carried out drying, degreasing and sintering, obtains porous niobium alloy material by foam impregnation method.Although porous niobium porosity prepared by the method is high, intensity is lower.
Summary of the invention
The object of the present invention is to provide a kind of method preparing lightweight Nb-Ti-Al based porous materials, be intended to prepare the lightweight niobium-base alloy with higher-strength, porosity and through-hole rate.
The present invention for raw material, adopts vacuum non-pressure sintering technique to prepare porous Nb-Ti-Al base alloy with mechanical alloying powder and rotating electrode atomized pre-alloyed powder.In mechanical alloying Nb-Ti-Al base alloy powder, Ti, Al element is evenly distributed in niobium matrix, and is solid-solution in niobium matrix and forms supersaturated solid solution.When sintering temperature is lower than Al fusing point, between Al and Nb, Ti and other alloying element, there is certain solid phase diffusion.After sintering temperature is more than Al fusing point, the flowing of aluminium liquid is sprawled and spreads in Nb, Ti fast, because the intrinsic diffusion coefficient of Al element is much larger than the intrinsic diffusion coefficient of Nb and Ti, Al causes Al original position to produce a large amount of hole to the inclined diffusion in Nb, Ti, and constantly gathering of hole just produces hole.Between Ti and Al, thermopositive reaction sharply can cause volumetric expansion.In order to suppress and control the expansion of porous insert, the spherical Nb-Ti-Al base pre-alloyed powder of single particle size prepared by rotating electrode atomized technique can be added in raw material powder.In sintering process, to form sintering neck, the inclined diffusion phenomena of Al element can not be there are, also can not form hole in pre-alloyed powder.After mixed powder sintering, local bonding between the pre-alloyed powder that particle diameter is larger also forms skeleton, limits the overplumping of mechanical alloying powder in poration process, effectively improves the intensity of porous insert.At heat treatment stages, Ti, Al element spreads further in Nb matrix, reaches equilibrium phase homogenization of composition.The present invention relies on the constituent element of reactant self to carry out pore-creating, and can prepare the porous niobium sill with higher-strength and Higher porosity, the hole in porous insert is interconnected, and solving between the intensity of porous niobium alloy and porosity can not the problem of matched well.This present invention is simple, and pore texture easily controls.
Prepare a method for lightweight Nb-Ti-Al based porous materials, concrete technology step has:
1, the preparation of mechanical alloying powder: weigh according to the composition proportion of mechanical alloying powder, raw material powder is-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites; Add the stearic acid of 0.5 ~ 2wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution.Ball during ball milling/material is than being (15 ~ 20)/1, and the rotating speed of ball mill is 350 ~ 500 revs/min, and Ball-milling Time is 24 ~ 72 hours, obtains the mechanical alloying powder that median size is 3 ~ 40 μm.
The composition of described mechanical alloying powder is: (27 ~ 40wt.%) Ti-(6 ~ 10wt.%) Al-(2 ~ 10wt.%) Cr-(1 ~ 6wt.%) W-(0.01 ~ 0.1wt.%) C-surplus Nb;
2, the mixing of mechanical alloying powder and atomized powder: mechanical alloying powder and rotating electrode atomized powder are mixed by ball milling.Rotating electrode atomized powder is single particle size distribution, and particle diameter is 60 ~ 150 μm, and weight percentage is 30 ~ 65%.Two kinds of powder mix 3 ~ 10 hours under the rotating speed of 200 ~ 300 revs/min, obtain mixed powder.
The composition of described rotating electrode atomized powder is: (20 ~ 26wt.%) Ti-(2 ~ 5wt.%) Al-(2 ~ 10wt.%) Cr-(1 ~ 6wt.%) W-(0.01 ~ 0.1wt.%) C-surplus Nb;
3, be shaped: in mixed powder, add 0.5 ~ 5wt.% dextrin or polyvinyl alcohol, at the Forming under Pressure of 300 ~ 800MPa, obtain pressed compact;
4, vacuum non-pressure sintering: pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 1 × 10
-3~ 4 × 10
-4start after Pa to heat up, with the ramp of 1 ~ 2 DEG C/min to 400 ~ 550 DEG C, insulation 20 ~ 60mim, then with the ramp of 0.2 ~ 0.5 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1500 ~ 1820 DEG C, be incubated 2 ~ 3 hours, obtain porous sintered base.
5, thermal treatment: porous sintered base carries out Homogenization Treatments at 1200 ~ 1600 DEG C, soaking time is 2 ~ 6 hours, obtains lightweight Nb-Ti-Al based porous materials.
The invention has the advantages that: the Kirkendall effect utilizing the inclined diffusion of Nb-Ti-Al base Al element to produce hole in the base carrys out pore-creating, form vesicular structure by the thermopositive reaction controlled between sintering temperature rise rate and preheating temperature control Al, Ti element in Reactive Synthesis process, and improve the intensity of porous material in conjunction with the sintering neck that atomized alloy powder is formed.Can by regulating mechanical alloying parameter, temperature rise rate, the particle diameter of atomized alloy powder and content and sintering temperature control porosity, pore size and void distribution state.This technological process is simple, flexible and convenient operation.The porosity of prepared lightweight niobium alloy porous material is 20 ~ 50%, and pore dimension is 20 ~ 500 μm, and compressive strength is between 60 ~ 300MPa.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is the microstructure of light porous niobium-base alloy.
Embodiment
Embodiment 1: porosity is the preparation of the lightweight Nb-Ti-Al based porous materials of 25%
With-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites for raw material, weigh according to the composition proportion of mechanical alloying powder.The composition of mechanical alloying powder is: 27wt.%Ti-6wt.%Al-2wt.%Cr-1wt.%W-0.02wt.%C-surplus Nb.Add the stearic acid of 0.5wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution.Ball/material is than being 15/1, and the rotating speed of ball mill is 500 revs/min, and Ball-milling Time is 36 hours, obtains the mechanical alloying powder that median size is 18 μm.Mechanical alloying powder and rotating electrode atomized powder are mixed by ball milling.The composition of rotating electrode atomized powder is 20wt.%Ti-2wt.%Al-2wt.%Cr-1wt.%W-0.02wt.%C-surplus Nb.Rotating electrode atomized powder is single particle size distribution, and particle diameter is 65 μm, and weight percentage is 30%.Two kinds of powder mix 7 hours under the rotating speed of 200 revs/min, obtain mixed powder.In mixed powder, add 0.5wt.% polyvinyl alcohol, at the Forming under Pressure of 300MPa, obtain pressed compact; Pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 2 × 10
-4start after Pa heat up, with the ramp of 1 DEG C/min to 550 DEG C, be incubated 60 minutes, then with the ramp of 0.5 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1815 DEG C, be incubated 2 hours, obtain porous sintered base.Porous sintered base carries out Homogenization Treatments at 1600 DEG C, and soaking time is 2 hours, obtains lightweight Nb-Ti-Al based porous materials.The porosity of porous material is 25%, and average pore size is 76 μm, and compressive strength is 286MPa.
Embodiment 2: porosity is the preparation of the lightweight Nb-Ti-Al based porous materials of 29%
With-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites for raw material, weigh according to the composition proportion of mechanical alloying powder.The composition of mechanical alloying powder is: 28wt.%Ti-8wt.%Al-4wt.%Cr-5wt.%) W-0.03wt.%C-surplus Nb.Add the stearic acid of 1wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution.Ball/material is than being 17/1, and the rotating speed of ball mill is 400 revs/min, and Ball-milling Time is 24 hours, obtains the mechanical alloying powder that median size is 32 μm.Mechanical alloying powder and rotating electrode atomized powder are passed through: 22wt.%Ti-3wt.%Al-4wt.%Cr-5wt.%W-0.03wt.%C-surplus Nb.Rotating electrode atomized powder is single particle size distribution, and particle diameter is 74 μm, and weight percentage is 65%.Two kinds of powder mix 6 hours under the rotating speed of 250 revs/min, obtain mixed powder.In mixed powder, add 1.5wt.% polyvinyl alcohol, at the Forming under Pressure of 400MPa, obtain pressed compact; Pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 2 × 10
-4start after Pa heat up, with the ramp of 1 DEG C/min to 500 DEG C, be incubated 40 minutes, then with the ramp of 0.4 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1700 DEG C, be incubated 2 hours, obtain porous sintered base.Porous sintered base carries out Homogenization Treatments at 1500 DEG C, and soaking time is 6 hours, obtains lightweight Nb-Ti-Al based porous materials.The porosity of porous material is 29%, and average pore size is 121 μm, and compressive strength is 251MPa.
Embodiment 3: porosity is the preparation of the lightweight Nb-Ti-Al based porous materials of 32%
With-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites for raw material, weigh according to the composition proportion of mechanical alloying powder.The composition of mechanical alloying powder is: 30wt.%Ti-8wt.%Al-6wt.%Cr-3wt.%) W-0.05wt.%C-surplus Nb.Add the stearic acid of 1.5wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution.Ball/material is than being 19/1, and the rotating speed of ball mill is 450 revs/min, and Ball-milling Time is 48 hours, obtains the mechanical alloying powder that median size is 27 μm.Mechanical alloying powder and rotating electrode atomized powder are mixed by ball milling.The composition of rotating electrode atomized powder is: 24wt.%Ti-4wt.%Al-6wt.%Cr-3wt.%) W-0.05wt.%C-surplus Nb.Rotating electrode atomized powder is single particle size distribution, and particle diameter is 102 μm, and weight percentage is 42%.Two kinds of powder mix 8 hours under the rotating speed of 300 revs/min, obtain mixed powder.In mixed powder, add 2.5wt.% dextrin, at the Forming under Pressure of 600MPa, obtain pressed compact; Pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 2 × 10
-4start after Pa heat up, with the ramp of 2 DEG C/min to 450 DEG C, be incubated 30 minutes, then with the ramp of 0.3 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1620 DEG C, be incubated 2.5 hours, obtain porous sintered base.Porous sintered base carries out Homogenization Treatments at 1400 DEG C, and soaking time is 4 hours, obtains lightweight Nb-Ti-Al based porous materials.The porosity of porous material is 32%, and average pore size is 278 μm, and compressive strength is 167MPa.
Embodiment 4: porosity is the preparation of the lightweight Nb-Ti-Al based porous materials of 43%
With-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites for raw material, weigh according to the composition proportion of mechanical alloying powder.The composition of mechanical alloying powder is: 36wt.%Ti-10wt.%Al-10wt.%Cr-1wt.%W-0.08wt.%C-surplus Nb.Add the stearic acid of 2wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution.Ball/material is than being 20/1, and the rotating speed of ball mill is 350 revs/min, and Ball-milling Time is 72 hours, obtains the mechanical alloying powder that median size is 40 μm.Mechanical alloying powder and rotating electrode atomized powder are mixed by ball milling.The composition of rotating electrode atomized powder is: 26wt.%Ti-5wt.%Al-10wt.%Cr-1wt.%W-0.08wt.%C-surplus Nb.Rotating electrode atomized powder is single particle size distribution, and particle diameter is 136 μm, and weight percentage is 50%.Two kinds of powder mix 10 hours under the rotating speed of 200 revs/min, obtain mixed powder.In mixed powder, add 5wt.% dextrin, at the Forming under Pressure of 800MPa, obtain pressed compact; Pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 2 × 10
-4start after Pa heat up, with the ramp of 1.5 DEG C/min to 400 DEG C, be incubated 20 minutes, then with the ramp of 0.2 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1520 DEG C, be incubated 3 hours, obtain porous sintered base.Porous sintered base carries out Homogenization Treatments at 1200 DEG C, and soaking time is 3 hours, obtains lightweight Nb-Ti-Al based porous materials.The porosity of porous material is 43%, and average pore size is 321 μm, and compressive strength is 65MPa.
Claims (4)
1. prepare a method for lightweight Nb-Ti-Al based porous materials, it is characterized in that:
Step one, weigh according to the composition proportion of mechanical alloying powder, raw material powder is-300 order niobium powder ,-300 order titanium valves ,-200 order aluminium powders ,-300 order chromium powders ,-500 order tungsten powders ,-500 order powdered graphites; Add the stearic acid of 0.5 ~ 2wt.% in addition in raw material powder after, pre-mixing is even, is then dispersed in niobium matrix by high-energy ball milling by various alloying element in high-purity Ar atmosphere, forms supersaturated solid solution; Ball during ball milling/material is than being (15 ~ 20)/1, and the rotating speed of ball mill is 350 ~ 500 revs/min, and Ball-milling Time is 24 ~ 72 hours, obtains the mechanical alloying powder that median size is 3 ~ 40 μm;
The mixing of step 2, mechanical alloying powder and atomized powder: mechanical alloying powder and rotating electrode atomized powder are mixed by ball milling; Rotating electrode atomized powder is single particle size distribution, and particle diameter is 60 ~ 150 μm, and weight percentage is 30 ~ 65%; Two kinds of powder mix 3 ~ 10 hours under the rotating speed of 200 ~ 300 revs/min, obtain mixed powder;
Step 3, in mixed powder, add 0.5 ~ 5wt.% dextrin or polyvinyl alcohol, at the Forming under Pressure of 300 ~ 800MPa, obtain pressed compact;
Step 4, pressed compact is placed in vacuum sintering furnace, vacuumizes.Treat that vacuum tightness reaches 1 × 10
-3~ 4 × 10
-4start after Pa to heat up, with the ramp of 1 ~ 2 DEG C/min to 400 ~ 550 DEG C, insulation 20-60 minute, then with the ramp of 0.2 ~ 0.5 DEG C/min to 700 DEG C, be incubated 60 minutes, then with the ramp of 10 DEG C/min to 1500-1820 DEG C, insulation 2-3 hour, obtains porous sintered base;
Step 5, porous sintered base carry out Homogenization Treatments at 1200 ~ 1600 DEG C, and soaking time is 2 ~ 6 hours, obtain lightweight Nb-Ti-Al based porous materials.
2. a kind of method preparing fine grain size and tabular alumina powder as claimed in claim 1, is characterized in that: the composition of the mechanical alloying powder described in step one is: (27 ~ 40wt.%) Ti-(6 ~ 10wt.%) Al-(2 ~ 10wt.%) Cr-(1 ~ 6wt.%) W-(0.01 ~ 0.1wt.%) C-surplus Nb.
3. a kind of method preparing fine grain size and tabular alumina powder as claimed in claim 1, is characterized in that: the composition of the rotating electrode atomized powder described in step 2 is: (20 ~ 26wt.%) Ti-(2 ~ 5wt.%) Al-(2 ~ 10wt.%) Cr-(1 ~ 6wt.%) W-(0.01 ~ 0.1wt.%) C-surplus Nb.
4. a kind of method preparing fine grain size and tabular alumina powder as claimed in claim 1, is characterized in that: the porosity of prepared lightweight Nb-Ti-Al based porous materials is 30-50%, and pore dimension is 20-500 μm, and compressive strength is between 60-300MPa.
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| CN106367633A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | La2O3-microalloyed TiAl-based alloy being high in acid corrosion resistance |
| CN106367624A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | Y-microalloyed TiAl-based alloy being high in acid corrosion resistance |
| CN109175360A (en) * | 2018-11-13 | 2019-01-11 | 武汉理工大学 | Preparation process based on powder sintering in-situ accomplishes high-manganses aluminum high-strength steel porous |
| CN109261968A (en) * | 2018-11-16 | 2019-01-25 | 攀枝花学院 | The preparation method of porous titanium or titanium alloy |
| CN111441007A (en) * | 2020-04-29 | 2020-07-24 | 安徽江南泵阀有限公司 | Treatment process for improving damage of fluid medium to mortar pump impeller |
| CN113427002A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工业大学 | Pressureless sintering preparation method of three-dimensional porous structure |
| CN115921874A (en) * | 2022-11-10 | 2023-04-07 | 长春工业大学 | TiAl-based composite material with two-stage reinforced three-dimensional network structure and preparation method thereof |
| CN118326222A (en) * | 2024-06-14 | 2024-07-12 | 西安稀有金属材料研究院有限公司 | High-performance composite binder phase hard alloy and preparation method thereof |
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| CN106367633A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | La2O3-microalloyed TiAl-based alloy being high in acid corrosion resistance |
| CN106367624A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | Y-microalloyed TiAl-based alloy being high in acid corrosion resistance |
| CN106367624B (en) * | 2016-09-12 | 2017-10-13 | 江苏大学 | High acid etching resistance Y microalloying TiAl-base alloys |
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| CN109175360B (en) * | 2018-11-13 | 2019-11-26 | 武汉理工大学 | Preparation process based on powder sintering in-situ accomplishes high-manganses aluminum high-strength steel porous |
| CN109261968A (en) * | 2018-11-16 | 2019-01-25 | 攀枝花学院 | The preparation method of porous titanium or titanium alloy |
| CN111441007A (en) * | 2020-04-29 | 2020-07-24 | 安徽江南泵阀有限公司 | Treatment process for improving damage of fluid medium to mortar pump impeller |
| CN111441007B (en) * | 2020-04-29 | 2023-09-01 | 安徽江南泵阀集团有限公司 | Treatment process for improving damage of fluid medium to mortar pump impeller |
| CN113427002A (en) * | 2021-06-25 | 2021-09-24 | 哈尔滨工业大学 | Pressureless sintering preparation method of three-dimensional porous structure |
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